CN100540612C - Preparation method of nano-magnetic ferrite particles and magnetic shock-absorbing rubber thereof - Google Patents
Preparation method of nano-magnetic ferrite particles and magnetic shock-absorbing rubber thereof Download PDFInfo
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- CN100540612C CN100540612C CNB2007101853834A CN200710185383A CN100540612C CN 100540612 C CN100540612 C CN 100540612C CN B2007101853834 A CNB2007101853834 A CN B2007101853834A CN 200710185383 A CN200710185383 A CN 200710185383A CN 100540612 C CN100540612 C CN 100540612C
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 95
- 239000002245 particle Substances 0.000 title claims abstract description 89
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 143
- 238000004073 vulcanization Methods 0.000 claims abstract description 90
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 244000043261 Hevea brasiliensis Species 0.000 claims abstract description 34
- 229920003052 natural elastomer Polymers 0.000 claims abstract description 34
- 229920001194 natural rubber Polymers 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 239000012744 reinforcing agent Substances 0.000 claims abstract 4
- 239000013543 active substance Substances 0.000 claims abstract 3
- 229920002943 EPDM rubber Polymers 0.000 claims abstract 2
- 238000002156 mixing Methods 0.000 claims description 38
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000002131 composite material Substances 0.000 claims description 20
- 230000007935 neutral effect Effects 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 2
- 239000012936 vulcanization activator Substances 0.000 claims 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 239000011593 sulfur Substances 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 238000013016 damping Methods 0.000 abstract description 40
- 230000000694 effects Effects 0.000 abstract description 11
- 239000006249 magnetic particle Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 230000035939 shock Effects 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000005728 strengthening Methods 0.000 description 38
- 229920001897 terpolymer Polymers 0.000 description 28
- 238000004458 analytical method Methods 0.000 description 22
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 13
- 238000012545 processing Methods 0.000 description 13
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 12
- -1 polyoxyethylene Polymers 0.000 description 12
- 238000005987 sulfurization reaction Methods 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 11
- 238000011010 flushing procedure Methods 0.000 description 11
- 239000002122 magnetic nanoparticle Substances 0.000 description 8
- 239000012798 spherical particle Substances 0.000 description 7
- 239000005864 Sulphur Substances 0.000 description 6
- 230000001737 promoting effect Effects 0.000 description 6
- 239000003223 protective agent Substances 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 3
- 230000037237 body shape Effects 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
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- 238000011049 filling Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
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- 238000003912 environmental pollution Methods 0.000 description 1
- 229920006335 epoxy glue Polymers 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229940087654 iron carbonyl Drugs 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Hard Magnetic Materials (AREA)
Abstract
本发明涉及磁性减震橡胶及纳米磁性铁氧粒子，具体为纳米磁性铁氧粒子的制备方法及利用该纳米磁性铁氧粒子制备的磁性减震橡胶。以解决现有磁性粒子无法满足磁性减震橡胶的物理力学性能与磁性减震效果以及现有磁性减震橡胶材料选择、配比不合理的问题。将1.4～5.11g的FeCl3·6H2O、1.75～6g的FeSO4·7H2O和分子量为400～10000的0.00025mol的聚乙二醇加入到560ml蒸馏水中并滴加氢氧化钠溶液而制得具有一定形貌并被聚乙二醇包覆的纳米磁性铁氧粒子。磁性减震橡胶由下列重量百分比的组分组成：天然橡胶15-60%，三元乙丙橡胶15-60%，纳米磁性铁氧粒子5-50%，硫化剂1-10%，硫化活性剂1-10%，硫化促进剂1-10%，防老剂0.1-5%，补强剂10-40%。The invention relates to magnetic shock-absorbing rubber and nano magnetic ferrite particles, in particular to a preparation method of nano magnetic ferrite particles and magnetic shock-absorbing rubber prepared by using the nano magnetic ferrite particles. In order to solve the problems that the existing magnetic particles cannot meet the physical and mechanical properties and the magnetic shock absorption effect of the magnetic shock-absorbing rubber, and the material selection and ratio of the existing magnetic shock-absorbing rubber are unreasonable. Add 1.4-5.11g of FeCl 3 6H 2 O, 1.75-6g of FeSO 4 7H 2 O and 0.00025mol polyethylene glycol with a molecular weight of 400-10000 into 560ml of distilled water and dropwise add sodium hydroxide solution to form Nano magnetic ferrite particles with certain shape and coated with polyethylene glycol are prepared. The magnetic damping rubber is composed of the following components by weight percentage: 15-60% natural rubber, 15-60% EPDM rubber, 5-50% nano-magnetic ferrite particles, 1-10% vulcanizing agent, and vulcanizing active agent 1-10%, vulcanization accelerator 1-10%, anti-aging agent 0.1-5%, reinforcing agent 10-40%.
Description
Technical field
The present invention relates to magnetic damping rubber and the used nano magnetic ferrite particle of preparation magnetic damping rubber, the magnetic damping rubber that is specially the preparation method of nano magnetic ferrite particle and utilizes this nano magnetic ferrite particle to prepare.
Background technology
The effect of vibroshock is to absorb vibrations and the impact that brings when vehicle jolts, reliable with the balance that assurance piggyback pod or engine are connected with drive disk assembly, kinetic force is normally transmitted safely, therefore, the quality of the performance of vehicle shock absorber own, have a strong impact on car load and occupant's comfortableness, also be related to the stationarity and the reliability of transmission of power between piggyback pod and the drive disk assembly, and influence the life-span of drive disk assembly and normally travelling of car load.
Magnetic rubber is the matrix material that is become according to certain processes by magnetic, rubber and Synergist S-421 95, have relative density little, be processed into advantages such as dimensional precision height and complicated shape goods easily, can overcome that original rigidity magneticsubstance (as: ferrite magnet, rare earth element magnet and alnico magnet etc.) is hard and crisp, poor in processability, can't make the defective of complexity and precise shape goods, so, with the gentle elasticity and the plasticity-of its uniqueness, be widely used in machinery, electronics, medical treatment, mine, the top science, military so that a plurality of fields such as articles for daily use.
The character of magnetic rubber uniqueness has determined it will have more wide application prospect in the cushioning material field.As the rubber phase ratio of cushioning material, the magnetic rubber cushioning material has more excellent heat and mechanical property, the more important thing is and can utilize its distinctive magnetic to resist external vibrations, thereby damping effect can improve greatly with generally.
At present, the matrix that is applied in the magnetic damping rubber mostly is natural rubber, and reason mainly is because natural rubber is cheap and easy to get, and has excellent curability and damping effect.But, the ageing-resistant performance of natural rubber, oil-proofness and high-and low-temperature resistance performance are all very poor, the magnetic damping rubber that makes is difficult to be applied in some high performance vibroshocks because not possessing high thermal stability, good physical and mechanical property and excellent damping effect simultaneously, and this has limited its Application Areas greatly; And be applied to magnetic particle in the magnetic damping rubber is iron carbonyl and the metal-powder that obtains by physical method mostly, generally has following defective: size distribution is very wide, size of particles forms not redispersible agglomerated particles easily and also needed to carry out chemical surface modification etc. before filling with the type looks are uncontrollable, be difficult to obtain nano level magnetic particle, made magnetic particle.These defectives cause the physical and mechanical property and the magnetic damping effect of the magnetic damping rubber for preparing to be difficult to reach service requirements, and magnetic property is difficult to control.And the filling quality ratio of its magnetic particle generally will reach more than 80% even 90%, and prescription so, and difficult forming, reduction property is poor, mechanical property is relatively low, damping effect is not good yet, thereby is difficult to be applied to the vibroshock field.
A kind of new technique as 21 century---the development of nanotechnology, also the research and development for magnetic damping rubber provide good basis.By the particle diameter and the form of control particle, be expected the excellent more magnetic nanoparticle of obtained performance, thereby prepare over-all properties excellent magnetism yielding rubber more.
Summary of the invention
The present invention provides a kind of preparation method of nano magnetic ferrite particle in order to solve the problem that existing magnetic particle can't satisfy the physical and mechanical property and the magnetic damping effect of magnetic damping rubber.This method is a kind of in-situ chemical method.
The present invention adopts following technical scheme to realize: the preparation method of nano magnetic ferrite particle, and with the FeCl of 1.4～5.11g
36H
2The FeSO of O, 1.75～6g
47H
2O and molecular weight are that the polyoxyethylene glycol of 400～10000 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 30～70 ℃, and be that the sodium hydroxide solution 40mL of 1.1～1.75mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 30～60 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, oven dry then must have controllable appearance and by the nano magnetic ferrite particle of coated with polyethylene glycol then.This product is carried out TEM, sreen analysis and infrared analysis, and it is the sphere of median size 5～30 nanometers as can be known, or bar-shaped or tetragonal body shape particle, and by coated with polyethylene glycol.
Reaction mechanism is as follows:
FeSO
4+2FeCl
3+8NaOH＝Fe
3O
4↓+Na
2SO
4+6NaCl+4H
2O
Magnetic particle among the present invention adopts the in-situ chemical method to make, its size distribution relative narrower, size (nano level) and the controlled (ball-type of pattern, bar-shaped or tetragonal body shape), the more important thing is: described preparation method just can realize the organic macromolecule finishing of its outside surface in the forming process of magnetic nanoparticle, thereby make made magnetic nanoparticle can not form not redispersible agglomerated particles, guarantee that directly adding made magnetic nanoparticle just can make the nano-magnetic yielding rubber, and, also provide assurance for the yielding rubber that obtains to have different physical and mechanical properties and magnetic property for making made nano-magnetic yielding rubber possess the excellent comprehensive physical and mechanical property simultaneously and magnetic property provides assurance.In addition, present method prepares the employed starting material (FeCl of magnetic nanoparticle
36H
2O, FeSO
47H
2O, polyoxyethylene glycol and sodium hydroxide) all cheap and easy to get, devices needed (common response still and agitator) is also very simple, and cheap, and reaction is medium with water and carries out under normal temperature, normal pressure, the basic non-environmental-pollution of preparation process, environment support equipment are also very simple.These characteristics all provide assurance for this preparation technology's industrialization and the popularization of industrialization and product.
Another object of the present invention provides the magnetic damping rubber that utilizes above-mentioned nano magnetic ferrite particle preparation, existing magnetic damping rubber material is selected to solve, proportioning, particularly body material selection and proportioning are unreasonable, and the used magnetic particle can't satisfy the problem of the physical and mechanical property and the magnetic damping effect of magnetic damping rubber.
Magnetic damping rubber of the present invention is to adopt following technical scheme to realize: magnetic damping rubber, form by following components in weight percentage: natural rubber 15-60%, terpolymer EP rubber 15-60%, nano magnetic ferrite particle 5-50%, vulcanizing agent 1-10%, vulcanization leveller 1-10%, vulcanization accelerator 1-10%, anti-aging agent 0.1-5%, strengthening agent 10-40%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.
The present invention is a matrix with the epoxy glue of terpolymer EP rubber and natural rubber, thereby make made nano-magnetic yielding rubber not only possess the ageing-resistant performance of terpolymer EP rubber excellence, oil-proofness and high-and low-temperature resistance, and possess excellent properties such as cheap and easy to get, excellent curability of natural rubber and damping effect.These characteristics make nano-magnetic yielding rubber of the present invention have more wide application prospect, not only can replace traditional rubber absorbers at present, but also can partly replace the metal vibroshock that use in some field.In addition, to be no more than 50% be its another characteristics for magnetic damping rubber of the present invention, the composition quality ratio of magnetic nanoparticle.Because the loading level of magnetic nanoparticle is no more than 50%, therefore be to be that external phase, magnetic nanoparticle are the matrix material of disperse phase with rubber, the magnetic damping rubber that makes the present invention obtain so not only possesses excellent formability, tailorability, mechanical characteristic etc., and possesses the excellent magnetism damping effect.This all can be smoothly provides assurance as the vibroshock in each field for this magnetic damping rubber.
Utilize the nano-magnetic rubber absorbers product of this proportioning raw materials, technological process and parameter preparation, analyze through means of testing such as mechanical property, magnetic property and electronic microscope photos, its tensile strength is not less than that 21.1MPa, tensile yield are about 413.0%, tear strength is not less than 62.0kN/m, shore hardness is 80, and magnetic induction reaches more than the 600GS; Particle aggregation is less, is tending towards homodisperse.
Embodiment
Embodiment 1
The preparation method of nano magnetic ferrite particle is with the FeCl of 1.4g
36H
2The FeSO of O, 1.75g
47H
2O and molecular weight are that the polyoxyethylene glycol of 400 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 30 ℃, and be that the sodium hydroxide solution 40mL of 1.1mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 30 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, and it is the rod-shaped particle of median size 12 * 45 nanometers as can be known, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 45%, nano magnetic ferrite particle 15%, vulcanizing agent 5%, vulcanization leveller 5%, vulcanization accelerator 4.9%, anti-aging agent 0.1%, strengthening agent 10%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.Described vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent can be selected the currently available products of various models.
Embodiment 2
The preparation method of nano magnetic ferrite particle is with the FeCl of 5.11g
36H
2The FeSO of O, 6g
47H
2O and molecular weight are that the polyoxyethylene glycol of 10000 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 70 ℃, and be that the sodium hydroxide solution 40mL of 1.75mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 60 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 18 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 60%, terpolymer EP rubber 15%, nano magnetic ferrite particle 5%, vulcanizing agent 3%, vulcanization leveller 2%, vulcanization accelerator 1%, anti-aging agent 4%, strengthening agent 10%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.For further optimizing product performance, vulcanizing agent adopts the composite vulcanizing agent of being made up of by 1: 1 mass ratio sulphur and vulcanizing agent DTDM; Vulcanization leveller adopts the composite sulfuration promoting agent of being made up of with 2: 3 mass ratio stearic acid and zinc oxide; Vulcanization accelerator adopts the composite sulfuration promotor of being made up of by 1: 1 mass ratio accelerator DM and vulcanization accelerator TT; Anti-aging agent is selected protective agent 4010 for use; Strengthening agent is selected carbon black for use.
Embodiment 3
The preparation method of nano magnetic ferrite particle is with the FeCl of 3.3g
36H
2The FeSO of O, 3.9g
47H
2O and molecular weight are that the polyoxyethylene glycol of 5000 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 50 ℃, and be that the sodium hydroxide solution 40mL of 1.4mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 45 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 20 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 35%, terpolymer EP rubber 30%, nano magnetic ferrite particle 5%, vulcanizing agent 1%, vulcanization leveller 6%, vulcanization accelerator 2%, anti-aging agent 1%, strengthening agent 20%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.Described vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent can be selected the currently available products of various models.
Embodiment 4
The preparation method of nano magnetic ferrite particle is with the FeCl of 2.5g
36H
2The FeSO of O, 2.8g
47H
2O and molecular weight are that the polyoxyethylene glycol of 1000 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 40 ℃, and be that the sodium hydroxide solution 40mL of 1.3mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 40 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the tetragonal body shape particle of median size 14 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 20%, terpolymer EP rubber 50%, nano magnetic ferrite particle 10%, vulcanizing agent 1%, vulcanization leveller 1%, vulcanization accelerator 1%, anti-aging agent 2%, strengthening agent 15%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.For further optimizing product performance, vulcanizing agent adopts the composite vulcanizing agent of being made up of by 1: 1 mass ratio sulphur and vulcanizing agent DTDM; Vulcanization leveller adopts the composite sulfuration promoting agent of being made up of with 2: 3 mass ratio stearic acid and zinc oxide; Vulcanization accelerator adopts the composite sulfuration promotor of being made up of by 1: 1 mass ratio accelerator DM and vulcanization accelerator TT; Anti-aging agent is selected protective agent 4010 for use; Strengthening agent is selected carbon black for use.
Embodiment 5
The preparation method of nano magnetic ferrite particle is with the FeCl of 4.5g
36H
2The FeSO of O, 5g
47H
2O and molecular weight are that the polyoxyethylene glycol of 8000 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 60 ℃, and be that the sodium hydroxide solution 40mL of 1.6mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 50 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 22 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 50%, terpolymer EP rubber 20%, nano magnetic ferrite particle 5%, vulcanizing agent 6%, vulcanization leveller 7%, vulcanization accelerator 1.5%, anti-aging agent 0.5%, strengthening agent 10%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.Described vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent can be selected the currently available products of various models.
Embodiment 6
The preparation method of nano magnetic ferrite particle is with the FeCl of 1.4g
36H
2The FeSO of O, 6g
47H
2O and molecular weight are the polyoxyethylene glycol of 2000 0.00025mol, join in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 35 ℃, and be that the sodium hydroxide solution 40mL of 1.5mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 35 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, places 40～60 ℃ baking oven to dry then, then gets nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 5 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 21%, terpolymer EP rubber 36%, nano magnetic ferrite particle 6%, vulcanizing agent 4%, vulcanization leveller 5%, vulcanization accelerator 4%, anti-aging agent 1%, strengthening agent 23%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.For further optimizing product performance, vulcanizing agent adopts the composite vulcanizing agent of being made up of by 1: 1 mass ratio sulphur and vulcanizing agent DTDM; Vulcanization leveller adopts the composite sulfuration promoting agent of being made up of with 2: 3 mass ratio stearic acid and zinc oxide; Vulcanization accelerator adopts the composite sulfuration promotor of being made up of by 1: 1 mass ratio accelerator DM and vulcanization accelerator TT; Anti-aging agent is selected protective agent 4010 for use; Strengthening agent is selected carbon black for use.
Embodiment 7
The preparation method of nano magnetic ferrite particle is with the FeCl of 5.11g
36H
2The FeSO of O, 1.75g
47H
2O and molecular weight are that the polyoxyethylene glycol of 800 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 45 ℃, and be that the sodium hydroxide solution 40mL of 1.2mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 55 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 28 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 60%, nano magnetic ferrite particle 5%, vulcanizing agent 7%, vulcanization leveller 1%, vulcanization accelerator 1%, anti-aging agent 1%, strengthening agent 10%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.Described vulcanizing agent, vulcanization accelerator, vulcanization leveller, anti-aging agent, strengthening agent can be selected the currently available products of various models.
Embodiment 8
The preparation method of nano magnetic ferrite particle is with the FeCl of 2g
36H
2The FeSO of O, 5.5g
47H
2O and molecular weight are that the polyoxyethylene glycol of 3000 0.00025mol joins in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 50 ℃, and be that the sodium hydroxide solution 40mL of 1.75mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 60 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, place 40～60 ℃ baking oven to dry then, then get nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 22 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 15%, nano magnetic ferrite particle 50%, vulcanizing agent 1%, vulcanization leveller 1%, vulcanization accelerator 7%, anti-aging agent 1%, strengthening agent 10%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.For further optimizing product performance, vulcanizing agent adopts the composite vulcanizing agent of being made up of by 1: 1 mass ratio sulphur and vulcanizing agent DTDM; Vulcanization leveller adopts the composite sulfuration promoting agent of being made up of with 2: 3 mass ratio stearic acid and zinc oxide; Vulcanization accelerator adopts the composite sulfuration promotor of being made up of by 1: 1 mass ratio accelerator DM and vulcanization accelerator TT; Anti-aging agent is selected protective agent 4010 for use; Strengthening agent is selected carbon black for use.
Embodiment 9
The preparation method of nano magnetic ferrite particle is with the FeCl of 5g
36H
2The FeSO of O, 4.5g
47H
2O and molecular weight are the polyoxyethylene glycol of 7000 0.00025mol, join in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 65 ℃, and be that the sodium hydroxide solution 40mL of 1.7mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 30 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, places 40～60 ℃ baking oven to dry then, then gets nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the spherical particle of median size 25 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 15%, nano magnetic ferrite particle 5%, vulcanizing agent 10%, vulcanization leveller 10%, vulcanization accelerator 2%, anti-aging agent 3%, strengthening agent 40%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.Described vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent can be selected the currently available products of various models.
Embodiment 10
The preparation method of nano magnetic ferrite particle is with the FeCl of 3g
36H
2The FeSO of O, 1.9g
47H
2O and molecular weight are the polyoxyethylene glycol of 600 0.00025mol, join in the 560ml distilled water, stirred 10 minutes, after mixing, gained solution is heated to 70 ℃, and be that the sodium hydroxide solution 40mL of 1.2mol/L is added drop-wise in the gained solution according to the rate of addition of 40 of per minutes with concentration, stirred 40 minutes to dripping the back fully, with methanol wash product (throw out), and then water flushing, until product is neutral, places 40～60 ℃ baking oven to dry then, then gets nano magnetic ferrite particle.This product is carried out TEM, sreen analysis and infrared analysis, learn that it is the rod-shaped particle of median size 10 * 40 nanometers, and by coated with polyethylene glycol.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 15%, nano magnetic ferrite particle 20%, vulcanizing agent 2%, vulcanization leveller 3%, vulcanization accelerator 10%, anti-aging agent 5%, strengthening agent 30%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.For further optimizing product performance, vulcanizing agent adopts the composite vulcanizing agent of being made up of by 1: 1 mass ratio sulphur and vulcanizing agent DTDM; Vulcanization leveller adopts the composite sulfuration promoting agent of being made up of with 2: 3 mass ratio stearic acid and zinc oxide; Vulcanization accelerator adopts the composite sulfuration promotor of being made up of by 1: 1 mass ratio accelerator DM and vulcanization accelerator TT; Anti-aging agent is selected protective agent 4010 for use; Strengthening agent is selected carbon black for use.
Embodiment 11
The preparation method of nano magnetic ferrite particle is identical with embodiment 1.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 15%, nano magnetic ferrite particle 30%, vulcanizing agent 1.2%, vulcanization leveller 1%, vulcanization accelerator 2%, anti-aging agent 0.8%, strengthening agent 35%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding the auxiliary agent and magnetic Nano iron oxygen particle that vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent, stearic acid and zinc oxide forms with 2: 3 mixed then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.Described vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent can be selected the currently available products of various models.
Embodiment 12
The preparation method of nano magnetic ferrite particle is identical with embodiment 5.
Utilize the magnetic damping rubber of above-mentioned nano magnetic ferrite particle preparation, form by following components in weight percentage: natural rubber 15%, terpolymer EP rubber 15%, nano magnetic ferrite particle 40%, vulcanizing agent 5%, vulcanization leveller 5%, vulcanization accelerator 5%, anti-aging agent 5%, strengthening agent 10%; With natural rubber, terpolymer EP rubber in proportion in mill normal temperature plasticate, after both are mixed, after adding vulcanizing agent, vulcanization leveller, vulcanization accelerator, anti-aging agent, strengthening agent and magnetic Nano iron oxygen particle then in proportion respectively, mixing, mixing even back is sheet down, and it is filled in the mould, on vulcanizing press according to 150 ℃ of temperature, pressure 125kgN/cm
2, time 20min processing parameter vulcanize, the demoulding then obtains the nano-magnetic yielding rubber.For further optimizing product performance, vulcanizing agent adopts the composite vulcanizing agent of being made up of by 1: 1 mass ratio sulphur and vulcanizing agent DTDM; Vulcanization leveller adopts the composite sulfuration promoting agent of being made up of with 2: 3 mass ratio stearic acid and zinc oxide; Vulcanization accelerator adopts the composite sulfuration promotor of being made up of by 1: 1 mass ratio accelerator DM and vulcanization accelerator TT; Anti-aging agent is selected protective agent 4010 for use; Strengthening agent is selected carbon black for use.
Claims (3)
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| CN103709462A (en) * | 2013-12-26 | 2014-04-09 | 金猴集团威海鞋业有限公司 | Rubber magnetic shoe sole pad and preparation method thereof |
| CN104212007A (en) * | 2014-08-27 | 2014-12-17 | 安徽微威胶件集团有限公司 | Magnetic damping rubber material and preparation method thereof |
| CN104877192B (en) * | 2015-06-03 | 2017-02-22 | 中北大学 | Fe3O4@GO/NR magnetic elastomer composite material and its preparation method |
| CN109354778A (en) * | 2018-09-19 | 2019-02-19 | 安徽卧龙泵阀股份有限公司 | A kind of rubber packing material preparation method of the modified montmorillonoid containing nano-magnetic powder |
| CN110684243A (en) * | 2019-09-26 | 2020-01-14 | 东莞市铭辉自动化设备有限公司 | Special rubber sleeve composition for grinding and polishing mobile phone glass |
| CN112953048A (en) * | 2021-02-18 | 2021-06-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Stator structure for weakening electromagnetic excitation force of motor |
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